関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Carbonochloridic acid, 3-chloropropyl ester | HCID 69399 | — |
| 反応物 | 3-Aminobenzyl alcohol | HCID 80293 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 3-Chloropropyl (3-hydroxymethylphenyl)carbamate | HCID 59564725 | — |
反応手順
3.7 g (30 mmol) of 3-aminobenzyl alcohol are dissolved in 50 ml of acetone, and 3.2 g (30 mmol) of sodium carbonate are added. 5.7 g (36 mmol) of 3-chloropropyl chloroformate are metered into this suspension at 25° C. The reaction mixture is stirred at room temperature for a further 18 h. Water is added to the reaction mixture for hydrolysis, and the solid is subsequently filtered off. The solution is concentrated by distillation, during which the product deposits as an oil. The product phase is separated off. The aqueous phase is extracted with ethyl acetate. The organic phases are combined, washed with water and dried over sodium sulfate. The mixture is subsequently evaporated to dryness. The crude product is reacted further directly without further purification;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08071593B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-5d8c0b52738e4576a6b5110ee3e74510 |
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| 出典メモ | uspto-grants-2011_12 |
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